WO2014119177A1 - Gas nozzle and plasma device employing same - Google Patents

Gas nozzle and plasma device employing same Download PDF

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Publication number
WO2014119177A1
WO2014119177A1 PCT/JP2013/084380 JP2013084380W WO2014119177A1 WO 2014119177 A1 WO2014119177 A1 WO 2014119177A1 JP 2013084380 W JP2013084380 W JP 2013084380W WO 2014119177 A1 WO2014119177 A1 WO 2014119177A1
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WO
WIPO (PCT)
Prior art keywords
region
gas nozzle
gas
sintered body
hole
Prior art date
Application number
PCT/JP2013/084380
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French (fr)
Japanese (ja)
Inventor
梶原　勇輝
Original Assignee
京セラ株式会社
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Publication date
Application filed by 京セラ株式会社 filed Critical 京セラ株式会社
Priority to JP2014559522A priority Critical patent/JP6046752B2/en
Priority to US14/763,106 priority patent/US9790596B1/en
Publication of WO2014119177A1 publication Critical patent/WO2014119177A1/en

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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45563—Gas nozzles
    • C—CHEMISTRY; METALLURGY
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    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45563—Gas nozzles
    • C23C16/45568—Porous nozzles
    • C—CHEMISTRY; METALLURGY
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    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45563—Gas nozzles
    • C23C16/45565—Shower nozzles
    • C—CHEMISTRY; METALLURGY
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    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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    • C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45587—Mechanical means for changing the gas flow
    • C23C16/45589—Movable means, e.g. fans
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/32431—Constructional details of the reactor
    • H01J37/3244—Gas supply means
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/32431—Constructional details of the reactor
    • H01J37/32458—Vessel
    • H01J37/32467—Material
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
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    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/32431—Constructional details of the reactor
    • H01J37/32458—Vessel
    • H01J37/32477—Vessel characterised by the means for protecting vessels or internal parts, e.g. coatings
    • H01J37/32495—Means for protecting the vessel against plasma
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
    • B05B1/00—Nozzles, spray heads or other outlets, with or without auxiliary devices such as valves, heating means
    • B05B1/14—Nozzles, spray heads or other outlets, with or without auxiliary devices such as valves, heating means with multiple outlet openings; with strainers in or outside the outlet opening
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B37/00—Lapping machines or devices; Accessories
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B37/00—Lapping machines or devices; Accessories
    • B24B37/04—Lapping machines or devices; Accessories designed for working plane surfaces
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C04B2235/9669—Resistance against chemicals, e.g. against molten glass or molten salts
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    • C04B35/03—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on magnesium oxide, calcium oxide or oxide mixtures derived from dolomite
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    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
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    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/4401—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber
    • C23C16/4404—Coatings or surface treatment on the inside of the reaction chamber or on parts thereof
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    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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    • C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber

Definitions

  • the present invention relates to a gas nozzle used in a plasma apparatus such as a film forming apparatus or an etching apparatus in a semiconductor manufacturing process or a liquid crystal manufacturing process, for example, and a plasma apparatus using the same.
  • a film forming apparatus for forming a thin film on an object such as a semiconductor wafer or a glass substrate or a plasma apparatus such as an etching apparatus for performing fine processing on the object. It has been.
  • a raw material gas is supplied into a reaction chamber, and this gas chemically reacts to form a thin film on the object.
  • a halogen-based corrosive gas is supplied as a raw material gas into the reaction chamber, and this gas is turned into plasma to become an etching gas, whereby the object is finely processed.
  • the plasma apparatus has a gas nozzle for supplying gas into the reaction chamber.
  • the gas nozzle includes a columnar body made of a ceramic sintered body in which a through hole through which a gas flows is formed.
  • the surface of the ceramic sintered body constituting the inner wall of the through hole is damaged when exposed to plasma gas in the reaction chamber, and particles may fall off from this surface. is there. When these particles adhere to the target object, the target object tends to be defective.
  • the present invention provides a gas nozzle that meets the demand of reducing particle dropout.
  • a gas nozzle includes a columnar body made of a ceramic sintered body in which a through hole through which a gas flows is formed. An outlet of the gas in the through hole is formed on one end surface of the main body.
  • the inner wall of the through hole has a first region located near the outlet and a second region located inside the main body with respect to the first region. Said 1st area
  • region consist of the baking surface of the said ceramic sintered compact.
  • the average crystal grain size in the first region is larger than the average crystal grain size in the second region.
  • a plasma apparatus includes a reaction chamber, the gas nozzle through which the gas flows into the reaction chamber, and a discharge member that converts the gas into plasma by discharge.
  • FIG. 1 It is sectional drawing of the film-forming apparatus using the gas nozzle by one Embodiment of this invention.
  • A is a perspective view of the gas nozzle shown in FIG. 1, and (b) is a cross-sectional view taken along line A1-A1 of (a).
  • A) And (b) is sectional drawing of the part corresponded to FIG.2 (b) which shows the manufacturing process of the gas nozzle shown in FIG.
  • A) And (b) is sectional drawing of the part corresponded to FIG.2 (b) which shows the manufacturing process of the gas nozzle shown in FIG.
  • a film forming apparatus 1 of this embodiment is an apparatus for forming a thin film on an object 2 such as a semiconductor wafer or a glass substrate by, for example, a plasma CVD method.
  • the film forming apparatus 1 includes a reaction chamber 3 in which an object 2 is accommodated and a film is formed on the object 2, a gas supply pipe 4 outside the reaction chamber 3 that supplies a raw material gas to the reaction chamber 3, A gas nozzle 5 in the reaction chamber 3 for supplying gas from the gas supply pipe 4 into the reaction chamber 3, and a holding member such as an electrostatic chuck on which the object 2 is placed in the reaction chamber 3 and an internal electrode 6 is provided.
  • the film forming apparatus 1 may further include a plate-like member having a flow path through which the gas flows, interposed between the gas supply pipe 4 and the gas nozzle 5.
  • the film forming apparatus 1 can form a thin film on the object 2 as follows, for example.
  • a raw material gas is supplied into the reaction chamber 3 from the gas supply pipe 4 through the gas nozzle 5.
  • the gas supplied into the reaction chamber 3 is turned into plasma above the object 2 by electric discharge from the coil 9 and the power supply 10.
  • the plasma gas atom or molecule is chemically reacted and deposited on the object 2 to form a thin film on the object 2.
  • SiO 2 silicon oxide
  • SiH 4 silane
  • Ar argon
  • oxygen (O 2 ) gas, and the like are supplied to the reaction chamber 3 as raw materials.
  • nitrogen trifluoride (NF 3 ) gas, octafluoropropane (C 3 F 8 ) gas, or the like is supplied to the reaction chamber 3 when unnecessary deposits are cleaned by plasma.
  • the gas nozzle 5 of this embodiment has a cylindrical main body 12 made of a ceramic sintered body in which a through hole 11 through which a gas flows is formed.
  • the main body 12 has an end surface 13 that is a lower surface, the other end surface 14 that is an upper surface, and a side surface 15 that is located between the one end surface 13 and the other end surface 14.
  • the diameter (width) of the main body 12 is, for example, 30 mm or more and 100 mm or less.
  • the height of the main body 12 is 30 mm or more and 100 mm or less, for example.
  • the main body 12 may be columnar, for example, polygonal columnar.
  • yttria (Y 2 O 3 ) sintered body As the ceramic sintered body of the main body 12, yttria (Y 2 O 3 ) sintered body, yttrium aluminum garnet (YAG) sintered body, for example, magnesium aluminate sintered body (MgAl 2 O 4 ) spinel firing It is desirable to use a sintered body or an alumina (Al 2 O 3 ) sintered body (hereinafter referred to as a high-purity alumina sintered body) having an alumina purity of 99.5% by mass or more. As a result, the plasma resistance of the ceramic sintered body can be improved.
  • the alumina purity is a content obtained by converting aluminum into an oxide in the alumina sintered body, and can be obtained as follows. First, a part of the alumina sintered body is pulverized, and the obtained powder is dissolved in a solution such as hydrochloric acid. Next, the dissolved solution is measured using an ICP (Inductively Coupled Plasma) emission spectroscopic analyzer (manufactured by Shimadzu Corporation: ICPS-8100, etc.). Thereby, the metal amount of each obtained component is converted into an oxide, and the alumina purity is obtained.
  • ICP Inductively Coupled Plasma
  • the main body 12 When the main body 12 is made of an yttria sintered body, it has higher plasma resistance than an yttrium / aluminum / garnet sintered body, a spinel sintered body, or a high-purity alumina sintered body. Therefore, damage to the main body 12 due to the plasma gas can be suppressed, so that the gas nozzle 5 can be used for a long period of time.
  • the yttria sintered body used for the main body 12 contains, for example, 99% by mass or more and 99.99% by mass or less of yttria as a main component, and 0. 0% of zirconium (Zr) or silicon (Si) as a sintering aid. It is contained in an amount of 01% by mass to 1% by mass.
  • content of each component in a yttria sintered compact is content which converted these into oxide, and can be calculated
  • the plasma resistance is not less than a certain level, and mechanical characteristics and thermal characteristics are excellent as compared with the yttria sintered body.
  • the spinel sintered body used for the main body 12 contains, for example, magnesium aluminate as a main component, for example, 90 mass% or more and 99.9 mass% or less, and calcium (Ca), magnesium (Mg), or zirconium is a sintering aid. As 0.1 mass% or more and 10 mass% or less. As a result, plasma resistance can be improved.
  • content of each component in a spinel sintered compact is content which converted these into the oxide, and can be calculated
  • the through-hole 11 may consist of only the first hole 18 or may further include a hole having a diameter different from that of the first hole 18 and the second hole 19.
  • the 1st hole part 18 and the 2nd hole part 19 should just be columnar shape, for example, may be polygonal columnar shape.
  • the longitudinal directions of the first hole 18 and the second hole 19 may be parallel to the longitudinal direction of the main body 12 or may not be parallel.
  • the inner wall of the first hole portion 18 is made of a sintered surface of a ceramic sintered body.
  • the burnt surface is a surface that has not been processed after the ceramic sintered body is obtained by firing and is still fired.
  • the inner wall of the first hole 18 has a first region 21 located near the outlet 16 and a second region 22 located inside the main body 12 rather than the first region 21.
  • the second region 22 of the present embodiment is a region other than the first region 21 in the first hole 18.
  • the inner wall of the second hole portion 19 is made of a processed surface such as a ground surface or a polished surface of a ceramic sintered body.
  • the ground surface is a surface on which grinding is performed after obtaining a ceramic sintered body by firing.
  • the polished surface is a surface that is subjected to grinding after the ceramic sintered body is obtained by firing, and further subjected to polishing.
  • the inner wall of the second hole 19 has a third region 23 located near the inflow port 17 and a fourth region 24 located inside the main body 12 more than the third region 23.
  • the fourth region 24 of the present embodiment is a region other than the third region 23 in the second hole 19.
  • it can confirm that the inner wall of the 2nd hole part 19 is a processed surface by observing the inner wall of the 2nd hole part 19 with a scanning electron microscope or a metal microscope.
  • the surface of the ceramic sintered body constituting the inner wall of the through hole 11 may be exposed to a plasma gas in the reaction chamber 3.
  • the average crystal grain size in the first region 21 is larger than the average crystal grain size in the second region 22.
  • the average crystal grain size on the surface of the ceramic sintered body is large, the ratio of the area on the surface of the sintered surface of the crystal grain boundary that is easily corroded by plasma decreases. For this reason, it becomes difficult for particles to fall off when the burnt skin surface is exposed to a plasma gas. Therefore, since it is located in the vicinity of the outlet 16, it is possible to satisfactorily reduce the generation of particles in the first region 21 that is more easily exposed to plasmad gas than the second region 22. Therefore, the adhesion of particles to the object 2 can be reduced, and the occurrence of defects in the object 2 can be suppressed.
  • the mechanical strength of the surface of the ceramic surface increases. Therefore, in the second region 22 which is located inside the main body 12 and is less exposed to the plasmad gas than the first region 21, the mechanical strength is increased while reducing the influence of the plasmad gas. Damage to the main body 12 due to mechanical stress or thermal stress can be suppressed.
  • the average crystal grain size in the first region 21 is desirably 1.5 times or more than the average crystal grain size in the second region 22. As a result, the generation of particles in the first region 21 can be favorably reduced. Further, the average crystal grain size in the first region 21 is desirably 10 times or less than the average crystal grain size in the second region 22. The average crystal grain size in the first region 21 is, for example, 3 ⁇ m or more and 20 ⁇ m or less. The average crystal grain size in the second region 22 is, for example, 2 ⁇ m or more and 10 ⁇ m or less.
  • the inner wall of the first hole portion 18 is a burnt surface
  • the inner wall of the second hole portion 19 is a processed surface such as a ground surface or a polished surface. Therefore, since the inner wall of the first hole 18 that is easily exposed to plasma gas because it is located on the outlet 16 side of the second hole 19 is made of a burnt surface, the generation of particles can be reduced well. Can do.
  • the second hole portion 19 can improve the accuracy of the position and shape by machining as compared with the case where the inner wall is made of a burnt surface.
  • the second hole portion 19 which is located on the inlet 17 side of the first hole portion 18 and is not easily exposed to plasma gas, the influence of the plasma gas is reduced, and the position and shape accuracy are increased. Further, gas leakage due to poor connection between the gas nozzle 5 and the gas supply pipe 4 can be suppressed.
  • the third region 23 located in the vicinity of the inflow port 17 is formed by a processing surface such as a grinding surface or a polishing surface, and thus is caused by poor connection between the gas nozzle 5 and the gas supply pipe 4. Gas leakage can be suppressed satisfactorily.
  • the third region 20 is preferably a region having a distance of 5 mm or less from the inflow port 17.
  • the one end surface 13 of the main body 12 is made of a sintered surface of a ceramic sintered body.
  • the one end face 13 that is easily exposed to plasma gas is a burnt surface, the generation of particles can be reduced satisfactorily.
  • the burnt surface is continuously formed from the one end surface 13 of the main body 12 to the first region 21 of the through hole 11. As a result, the generation of particles can be reduced favorably.
  • the one end surface 13 may be a processed surface such as a ground surface or a polished surface. In this case, it is desirable that the one end surface 13 is a polished surface from the viewpoint of suppressing the falling off of the particles.
  • the other end surface 14 of the main body 12 is preferably made of a ground surface or a polished surface of a ceramic sintered body.
  • a main body sintered body 25 which is a ceramic sintered body before the through hole 11 of the main body 12 is formed is prepared. Specifically, for example, the following is performed.
  • pure water and an organic binder are added to the ceramic powder, and then wet mixed with a ball mill to prepare a slurry.
  • the slurry is granulated by spray drying to form a ceramic powder.
  • the ceramic powder is molded into a predetermined shape using a molding method such as a die pressing method or a cold isostatic pressing method (CIP molding method), and the cylindrical shape shown in FIG.
  • the molded body 26 is obtained.
  • a recess 27 that opens to the one end surface 13 that forms the first hole 18 described above is formed in the molded body 26 by cutting.
  • firing is performed at, for example, 1400 ° C. or more and 2000 ° C.
  • the molded body 26 is fired by placing the molded body 26 on the mounting table 28 of the firing furnace while exposing the one end surface 13 with the recess 27 opened as an upper side. It is done in the state.
  • the inner wall of the recess 27 has a first region 21 located near the one end surface 13 in the first region 21 than the first region 21. Compared with the second region 22 located inside the molded body 26, large heat is likely to be applied.
  • the molded body 26 is fired. Liquid phase sintering occurs. For this reason, the crystal of the first region 21 to which heat larger than that of the second region 22 is applied is likely to grow larger than that of the second region 22. As a result, the average crystal grain size in the first region 21 can be made larger than the average crystal grain size in the second region 22 on the inner wall of the recess 27 of the main body sintered body 25.
  • the first hole 18 having a diameter as small as 0.1 mm or more and 2 mm or less it is necessary to reduce the diameter of the recess 27 serving as the first hole 18. It becomes difficult to flow. Therefore, when the molded body 26 is baked, the heat applied to the inner wall of the recess 27 is likely to be uneven, and the heat applied to the first region 21 is likely to be greater than the heat applied to the second region 22. Therefore, the average crystal grain size in the first region 21 is likely to be larger than the average crystal grain size in the second region 22 on the inner wall of the recess 27 of the main body sintered body 25.
  • the recess 27 has a bottom surface at the end opposite to the one end surface 13 and does not penetrate the main body 12. As a result, it becomes difficult for air to flow in the recess 27. Therefore, the average crystal grain size in the first region 21 is likely to be larger than the average crystal grain size in the second region 22 on the inner wall of the recess 27 of the main body sintered body 25.
  • the molded body 26 As a molding method for forming the molded body 26, it is desirable to use a CIP molding method. According to the CIP molding method, since the pressure during molding is uniformly applied, the density of the molded body 26 can be made uniform. Therefore, when the molded body 26 is fired, crystal grains grow uniformly according to the applied temperature. As described above, the first region 21 is heated by applying heat larger than that of the second region 22 to the first region 21. The average crystal grain size in 21 is easily made larger than the average crystal grain size in the second region 22.
  • Hole processing is performed from the other end surface 14 side of the main body sintered body 25 using grinding, and the second hole portion 19 that opens to the other end surface 14 and is connected to the recess 27 is formed in the main body sintered body 25. . Accordingly, the recess 27 becomes the first hole 18, and the through-hole 11 constituted by the first hole 18 and the second hole 19 can be formed. Moreover, the other end surface 14 is ground by using a grinding process to obtain a ground surface. As a result, the main body sintered body 25 can be the main body 12. In addition, you may use ultrasonic processing as a grinding process.
  • the one end surface 13 can be made to be a burnt skin surface by not performing processing such as grinding or polishing on the one end surface 13.
  • the grilled surface is continuously formed from the one end surface 13 of the main body 12 to the first region 21 of the through hole 11.
  • the end surface 13 may be subjected to processing such as grinding or polishing.
  • the processing amount along the longitudinal direction of the main body sintered body 25 is desirably, for example, not less than 0.5 mm and not more than 2 mm. As a result, the first region 21 can remain in the main body 12.
  • the inner wall of the second hole 19 becomes a ground surface.
  • the inner wall of the 2nd hole part 19 can be made into a grinding
  • the other end surface 14 can be used as a polishing surface by polishing the other end surface 14.
  • the configuration in which the gas nozzle is used in the film forming apparatus has been described as an example.
  • the gas nozzle may be used in another semiconductor manufacturing apparatus or liquid crystal manufacturing apparatus, for example, an etching apparatus.

Abstract

A gas nozzle according to an embodiment of the present invention comprises a columnar main body formed from a ceramic sintered body, whereupon through holes are formed wherethrough gas flows. Gas discharge apertures in the through holes are formed on one end face of the main body. Inner walls of the through holes further comprise first regions which are located near the discharge apertures, and second regions which are located further inward of the main body than the first regions. The first regions and the second regions are formed from an untreated face of the ceramic sintered body. Average crystal grain diameters in the first regions are greater than average crystal grain diameters in the second regions.

Description

ガスノズルおよびこれを用いたプラズマ装置Gas nozzle and plasma apparatus using the same
　本発明は、例えば半導体製造工程または液晶製造工程において、例えば成膜装置またはエッチング装置などのプラズマ装置に用いられるガスノズルおよびこれを用いたプラズマ装置に関するものである。 The present invention relates to a gas nozzle used in a plasma apparatus such as a film forming apparatus or an etching apparatus in a semiconductor manufacturing process or a liquid crystal manufacturing process, for example, and a plasma apparatus using the same.
　従来、半導体製造工程または液晶製造工程においては、半導体ウエハまたはガラス基板などの対象物に薄膜を成膜するための成膜装置または対象物に微細加工を施すためのエッチング装置などのプラズマ装置が用いられている。成膜装置では、原料のガスが反応室内に供給され、このガスが化学反応することによって、対象物上に薄膜が形成される。また、エッチング装置では、原料のガスとしてハロゲン系腐食性ガスが反応室内に供給され、このガスがプラズマ化してエッチングガスとなることによって、対象物に微細加工が施される。 Conventionally, in a semiconductor manufacturing process or a liquid crystal manufacturing process, a film forming apparatus for forming a thin film on an object such as a semiconductor wafer or a glass substrate or a plasma apparatus such as an etching apparatus for performing fine processing on the object is used. It has been. In the film forming apparatus, a raw material gas is supplied into a reaction chamber, and this gas chemically reacts to form a thin film on the object. In the etching apparatus, a halogen-based corrosive gas is supplied as a raw material gas into the reaction chamber, and this gas is turned into plasma to become an etching gas, whereby the object is finely processed.
　特開２０００－１９５８０７号公報に開示されているように、プラズマ装置は、ガスを反応室内に供給するためのガスノズルを有している。このガスノズルは、ガスが流れる貫通孔が形成されたセラミック焼結体からなる柱状の本体を備えている。 As disclosed in Japanese Patent Laid-Open No. 2000-195807, the plasma apparatus has a gas nozzle for supplying gas into the reaction chamber. The gas nozzle includes a columnar body made of a ceramic sintered body in which a through hole through which a gas flows is formed.
　ところで、プラズマ装置を用いる際に、貫通孔の内壁を構成するセラミック焼結体の表面が、反応室内でプラズマ化したガスに晒されると損傷を受けてしまい、この表面からパーティクルが脱落することがある。このパーティクルが対象物に付着すると、対象物に不良が生じやすくなる。 By the way, when using the plasma apparatus, the surface of the ceramic sintered body constituting the inner wall of the through hole is damaged when exposed to plasma gas in the reaction chamber, and particles may fall off from this surface. is there. When these particles adhere to the target object, the target object tends to be defective.
　本発明は、パーティクルの脱落を低減する要求に応えるガスノズルを提供するものである。 The present invention provides a gas nozzle that meets the demand of reducing particle dropout.
　本発明の一形態によるガスノズルは、ガスが流れる貫通孔が形成されたセラミック焼結体からなる柱状の本体を備える。該本体の一端面には、前記貫通孔における前記ガスの流出口が形成されている。前記貫通孔の内壁は、前記流出口の近傍に位置する第１領域と該第１領域よりも前記本体の内部に位置する第２領域とを有する。前記第１領域および前記第２領域は、前記セラミック焼結体の焼き肌面からなる。前記第１領域における平均結晶粒径は、前記第２領域における平均結晶粒径よりも大きい。 A gas nozzle according to an embodiment of the present invention includes a columnar body made of a ceramic sintered body in which a through hole through which a gas flows is formed. An outlet of the gas in the through hole is formed on one end surface of the main body. The inner wall of the through hole has a first region located near the outlet and a second region located inside the main body with respect to the first region. Said 1st area | region and said 2nd area | region consist of the baking surface of the said ceramic sintered compact. The average crystal grain size in the first region is larger than the average crystal grain size in the second region.
　本発明の一形態によるプラズマ装置は、反応室と、該反応室内に前記ガスが流出する上記ガスノズルと、前記ガスを放電によってプラズマ化させる放電部材とを備える。 A plasma apparatus according to an aspect of the present invention includes a reaction chamber, the gas nozzle through which the gas flows into the reaction chamber, and a discharge member that converts the gas into plasma by discharge.
　本発明の一形態によるガスノズルによれば、プラズマ化したガスに晒されやすい第１領域における耐プラズマ性を高め、ひいてはパーティクルの脱落を低減することができる。 According to the gas nozzle of one embodiment of the present invention, it is possible to improve the plasma resistance in the first region that is easily exposed to the plasma gas, and to reduce the dropout of particles.
本発明の一実施形態によるガスノズルを用いた成膜装置の断面図である。It is sectional drawing of the film-forming apparatus using the gas nozzle by one Embodiment of this invention. （ａ）は、図１に示したガスノズルの斜視図であり、（ｂ）は、（ａ）のＡ１－Ａ１線における断面図である。(A) is a perspective view of the gas nozzle shown in FIG. 1, and (b) is a cross-sectional view taken along line A1-A1 of (a). （ａ）および（ｂ）は、図１に示したガスノズルの製造工程を示す、図２（ｂ）に相当する部分の断面図である。(A) And (b) is sectional drawing of the part corresponded to FIG.2 (b) which shows the manufacturing process of the gas nozzle shown in FIG. （ａ）および（ｂ）は、図１に示したガスノズルの製造工程を示す、図２（ｂ）に相当する部分の断面図である。(A) And (b) is sectional drawing of the part corresponded to FIG.2 (b) which shows the manufacturing process of the gas nozzle shown in FIG.
　＜ガスノズル＞
  以下に、本発明の一実施形態によるガスノズルを用いた成膜装置１について、図１および図２を参照して詳細に説明する。 <Gas nozzle>
Hereinafter, a film forming apparatus 1 using a gas nozzle according to an embodiment of the present invention will be described in detail with reference to FIGS. 1 and 2.
　図１に示すように、本実施形態の成膜装置１は、例えばプラズマＣＶＤ法によって半導体ウェハまたはガラス基板などの対象物２に薄膜を成膜する装置である。成膜装置１は、対象物２が収容されるとともに対象物２への成膜が行なわれる反応室３と、反応室３に原料のガスを供給する反応室３外部のガス供給管４と、ガス供給管４から反応室３内にガスを供給する反応室３内のガスノズル５と、反応室３内で対象物２が載置されるとともに内部電極６を備えた静電チャックなどの保持部材７と、内部電極６が電気的に接続される反応室３外部のバイアス電源８と、反応室３内にプラズマを生成するために反応室３外部に設けられた放電部材とを備えている。この放電部材は、コイル９および電源１０によって構成されており、原料ガスが供給された反応室３内において放電を行なう。なお、成膜装置１は、ガス供給管４とガスノズル５との間に介在した、ガスが流れる流路を有する板状部材をさらに備えていてもよい。 As shown in FIG. 1, a film forming apparatus 1 of this embodiment is an apparatus for forming a thin film on an object 2 such as a semiconductor wafer or a glass substrate by, for example, a plasma CVD method. The film forming apparatus 1 includes a reaction chamber 3 in which an object 2 is accommodated and a film is formed on the object 2, a gas supply pipe 4 outside the reaction chamber 3 that supplies a raw material gas to the reaction chamber 3, A gas nozzle 5 in the reaction chamber 3 for supplying gas from the gas supply pipe 4 into the reaction chamber 3, and a holding member such as an electrostatic chuck on which the object 2 is placed in the reaction chamber 3 and an internal electrode 6 is provided. 7, a bias power supply 8 outside the reaction chamber 3 to which the internal electrode 6 is electrically connected, and a discharge member provided outside the reaction chamber 3 for generating plasma in the reaction chamber 3. This discharge member is constituted by a coil 9 and a power source 10, and discharges in the reaction chamber 3 to which the raw material gas is supplied. The film forming apparatus 1 may further include a plate-like member having a flow path through which the gas flows, interposed between the gas supply pipe 4 and the gas nozzle 5.
　この成膜装置１は、例えば以下のようにして、対象物２に薄膜を成膜することができる。ガス供給管４からガスノズル５を介して反応室３内に原料のガスを供給する。反応室３内に供給されたガスは、対象物２の上方において、コイル９および電源１０から供給された電力による放電によってプラズマ化する。このプラズマ化したガスの原子または分子が化学反応して対象物２に堆積することによって、対象物２に薄膜が成膜される。例えば、対象物２上に酸化ケイ素（ＳｉＯ２）薄膜を形成するときは、シラン（ＳｉＨ４）ガス、アルゴン（Ａｒ）ガス、および酸素（Ｏ２）ガス等が原料として反応室３に供給される。なお、プラズマによって不要堆積物をクリーニングするときは、三フッ化窒素（ＮＦ３）ガス、またはオクタフルオロプロパン（Ｃ３Ｆ８）ガス等が反応室３に供給される。 The film forming apparatus 1 can form a thin film on the object 2 as follows, for example. A raw material gas is supplied into the reaction chamber 3 from the gas supply pipe 4 through the gas nozzle 5. The gas supplied into the reaction chamber 3 is turned into plasma above the object 2 by electric discharge from the coil 9 and the power supply 10. The plasma gas atom or molecule is chemically reacted and deposited on the object 2 to form a thin film on the object 2. For example, when a silicon oxide (SiO 2 ) thin film is formed on the target 2, silane (SiH 4 ) gas, argon (Ar) gas, oxygen (O 2 ) gas, and the like are supplied to the reaction chamber 3 as raw materials. The Note that nitrogen trifluoride (NF 3 ) gas, octafluoropropane (C 3 F 8 ) gas, or the like is supplied to the reaction chamber 3 when unnecessary deposits are cleaned by plasma.
　次に、本実施形態のガスノズル５について詳細に説明する。図２（ａ）および（ｂ）に示すように、ガスノズル５は、ガスが流れる貫通孔１１が形成されたセラミック焼結体からなる円柱状の本体１２を有する。この本体１２は、下面である一端面１３と、上面である他端面１４と、一端面１３および他端面１４の間に位置する側面１５とを有する。本体１２の直径（幅）は、例えば３０ｍｍ以上１００ｍｍ以下である。また、本体１２の高さは、例えば３０ｍｍ以上１００ｍｍ以下である。なお、本体１２は、柱状であればよく、例えば多角柱状であってもよい。 Next, the gas nozzle 5 of this embodiment will be described in detail. As shown in FIGS. 2A and 2B, the gas nozzle 5 has a cylindrical main body 12 made of a ceramic sintered body in which a through hole 11 through which a gas flows is formed. The main body 12 has an end surface 13 that is a lower surface, the other end surface 14 that is an upper surface, and a side surface 15 that is located between the one end surface 13 and the other end surface 14. The diameter (width) of the main body 12 is, for example, 30 mm or more and 100 mm or less. Moreover, the height of the main body 12 is 30 mm or more and 100 mm or less, for example. The main body 12 may be columnar, for example, polygonal columnar.
　ガスノズル５の本体１２は、セラミック焼結体からなるため、耐プラズマ性が高い。その結果、本体１２が反応室３内のプラズマ化したガスに晒された際に、本体１２からパーティクルの発生を低減することができる。したがって、対象物２へのパーティクルの付着を低減することができ、対象物２における不良の発生を抑制することができる。 Since the main body 12 of the gas nozzle 5 is made of a ceramic sintered body, it has high plasma resistance. As a result, generation of particles from the main body 12 can be reduced when the main body 12 is exposed to the plasmad gas in the reaction chamber 3. Therefore, the adhesion of particles to the object 2 can be reduced, and the occurrence of defects in the object 2 can be suppressed.
　本体１２のセラミック焼結体としては、イットリア（Ｙ２Ｏ３）焼結体、イットリウム・アルミニウム・ガーネット（ＹＡＧ）焼結体、例えばアルミン酸マグネシウム焼結体（ＭｇＡｌ２Ｏ４）であるスピネル焼結体またはアルミナ純度が９９．５質量％以上であるアルミナ（Ａｌ２Ｏ３）焼結体（以下、高純度アルミナ焼結体という）などを用いることが望ましい。その結果、セラミック焼結体の耐プラズマ性を高めることができる。 As the ceramic sintered body of the main body 12, yttria (Y 2 O 3 ) sintered body, yttrium aluminum garnet (YAG) sintered body, for example, magnesium aluminate sintered body (MgAl 2 O 4 ) spinel firing It is desirable to use a sintered body or an alumina (Al 2 O 3 ) sintered body (hereinafter referred to as a high-purity alumina sintered body) having an alumina purity of 99.5% by mass or more. As a result, the plasma resistance of the ceramic sintered body can be improved.
　なお、アルミナ純度は、アルミナ焼結体においてアルミニウムを酸化物に換算した含有量のことであり、以下のようにして求めることができる。まず、アルミナ焼結体の一部を粉砕し、得られた粉体を塩酸などの溶液に溶解する。次に、ＩＣＰ（Inductively Coupled Plasma）発光分光分析装置（島津製作所製：ＩＣＰＳ－8100等）を用いて、溶解した溶液を測定する。これによって、得られた各成分の金属量を酸化物に換算し、アルミナ純度を求める。 The alumina purity is a content obtained by converting aluminum into an oxide in the alumina sintered body, and can be obtained as follows. First, a part of the alumina sintered body is pulverized, and the obtained powder is dissolved in a solution such as hydrochloric acid. Next, the dissolved solution is measured using an ICP (Inductively Coupled Plasma) emission spectroscopic analyzer (manufactured by Shimadzu Corporation: ICPS-8100, etc.). Thereby, the metal amount of each obtained component is converted into an oxide, and the alumina purity is obtained.
　本体１２がイットリア焼結体からなる場合には、イットリウム・アルミニウム・ガーネット焼結体、スピネル焼結体または高純度アルミナ焼結体と比較して耐プラズマ性が高い。したがって、プラズマ化したガスによる本体１２の損傷を抑制できるため、ガスノズル５を長期間に渡って使用することができる。本体１２に用いられるイットリア焼結体は、例えば、イットリアを主成分として例えば９９質量％以上９９．９９質量％以下含んでおり、ジルコニウム（Ｚｒ）またはシリコン（Ｓｉ）を焼結助剤として０．０１質量％以上１質量％以下含んでいる。なお、イットリア焼結体における各成分の含有量は、これらを酸化物に換算した含有量のことであり、前述したアルミナ純度と同様にＩＣＰ発光分光分析装置を用いて求めることができる。 When the main body 12 is made of an yttria sintered body, it has higher plasma resistance than an yttrium / aluminum / garnet sintered body, a spinel sintered body, or a high-purity alumina sintered body. Therefore, damage to the main body 12 due to the plasma gas can be suppressed, so that the gas nozzle 5 can be used for a long period of time. The yttria sintered body used for the main body 12 contains, for example, 99% by mass or more and 99.99% by mass or less of yttria as a main component, and 0. 0% of zirconium (Zr) or silicon (Si) as a sintering aid. It is contained in an amount of 01% by mass to 1% by mass. In addition, content of each component in a yttria sintered compact is content which converted these into oxide, and can be calculated | required using an ICP emission-spectral-analysis apparatus similarly to the alumina purity mentioned above.
　また、本体１２がスピネル焼結体からなる場合には、耐プラズマ性が一定以上あるとともに、イットリア焼結体と比較して機械的特性および熱的特性が優れている。本体１２に用いられるスピネル焼結体は、例えばアルミン酸マグネシウムを主成分として例えば９０質量％以上９９．９質量％以下含んでおり、カルシウム（Ｃａ）、マグネシウム（Ｍｇ）またはジルコニウムを焼結助剤として０．１質量％以上１０質量％以下含んでいる。その結果、耐プラズマ性を高めることができる。また、スピネル焼結体における各成分の含有量は、これらを酸化物に換算した含有量のことであり、前述したアルミナ純度と同様にＩＣＰ発光分光分析装置を用いて求めることができる。 Further, when the main body 12 is made of a spinel sintered body, the plasma resistance is not less than a certain level, and mechanical characteristics and thermal characteristics are excellent as compared with the yttria sintered body. The spinel sintered body used for the main body 12 contains, for example, magnesium aluminate as a main component, for example, 90 mass% or more and 99.9 mass% or less, and calcium (Ca), magnesium (Mg), or zirconium is a sintering aid. As 0.1 mass% or more and 10 mass% or less. As a result, plasma resistance can be improved. Moreover, content of each component in a spinel sintered compact is content which converted these into the oxide, and can be calculated | required using an ICP emission-spectral-analysis apparatus similarly to the alumina purity mentioned above.
　また、本体１２がイットリウム・アルミニウム・ガーネット焼結体からなる場合には、耐プラズマ性が一定以上であるとともに、イットリア焼結体やスピネル焼結体と比較して機械的特性および熱的特性が優れている。本体１２に用いられるＹＡＧ焼結体は、イットリアを例えば４５ｍｏｌ％以上８０ｍｏｌ％以下含んでおり、アルミナを例えば２０ｍｏｌ％以上５５ｍｏｌ％以下含んでいる。その結果、機械的特性を優れたものとするとともに耐プラズマ性を高めることができる。なお、イットリウム・アルミニウム・ガーネット焼結体に含まれる各成分の含有量は、これらを酸化物に換算した含有量のことであり、前述したアルミナ純度と同様にＩＣＰ発光分光分析装置を用いて求めることができる。 When the main body 12 is made of a yttrium / aluminum / garnet sintered body, the plasma resistance is not less than a certain level, and mechanical and thermal characteristics are higher than those of the yttria sintered body and the spinel sintered body. Are better. The YAG sintered compact used for the main body 12 contains yttria, for example, at 45 mol% or more and 80 mol% or less, and alumina, for example, at 20 mol% or more and 55 mol% or less. As a result, the mechanical properties can be improved and the plasma resistance can be improved. The content of each component contained in the sintered body of yttrium / aluminum / garnet is a content obtained by converting these into oxides, and is obtained using an ICP emission spectroscopic analyzer in the same manner as the alumina purity described above. be able to.
　本体１２に形成された貫通孔１１は、ガスノズル５においてガスが流れる流路である。この貫通孔１１は、一端面１３に形成された、ガスを反応室３内へ流出する流出口１６と、他端面１４に形成された、ガス供給管４からガスが流入する流入口１７とを有する。 The through hole 11 formed in the main body 12 is a flow path through which gas flows in the gas nozzle 5. This through hole 11 has an outlet 16 formed on one end face 13 for flowing gas into the reaction chamber 3, and an inlet 17 formed on the other end face 14 for flowing gas from the gas supply pipe 4. Have.
　また、貫通孔１１は、流出口１６側に配された円柱状の第１孔部１８と、流入口１７側に配された円柱状の第２孔部１９とを有する。第１孔部１８の直径（幅）は、第２孔部１９の直径（幅）よりも小さい。第１孔部１８の直径（幅）は、例えば０．１ｍｍ以上２ｍｍ以下である。第１孔部１８の高さは、例えば１ｍｍ以上１０ｍｍ以下である。第２孔部１９の直径（幅）は、例えば１ｍｍ以上２０ｍｍ以下である。第２孔部１９の高さは、例えば１０ｍｍ以上１００ｍｍ以下である。なお、貫通孔１１は、第１孔部１８のみからなってもよいし、第１孔部１８および第２孔部１９と異なる直径の孔部をさらに有していてもよい。また、第１孔部１８および第２孔部１９は、柱状であればよく、例えば多角柱状であってもよい。また、第１孔部１８および第２孔部１９の長手方向は、本体１２の長手方向と平行であってもよいし、平行でなくてもよい。 Further, the through hole 11 has a columnar first hole 18 disposed on the outlet 16 side and a columnar second hole 19 disposed on the inlet 17 side. The diameter (width) of the first hole 18 is smaller than the diameter (width) of the second hole 19. The diameter (width) of the first hole 18 is, for example, not less than 0.1 mm and not more than 2 mm. The height of the 1st hole 18 is 1 mm or more and 10 mm or less, for example. The diameter (width) of the second hole 19 is, for example, 1 mm or more and 20 mm or less. The height of the second hole 19 is, for example, not less than 10 mm and not more than 100 mm. The through-hole 11 may consist of only the first hole 18 or may further include a hole having a diameter different from that of the first hole 18 and the second hole 19. Moreover, the 1st hole part 18 and the 2nd hole part 19 should just be columnar shape, for example, may be polygonal columnar shape. The longitudinal directions of the first hole 18 and the second hole 19 may be parallel to the longitudinal direction of the main body 12 or may not be parallel.
　第１孔部１８と第２孔部１９との境界には、第１孔部１８の内壁と第２孔部１０の内壁とを接続する段差部２０が形成されている。その結果、第２孔部１９の内壁でパーティクルが発生したとしても、段差部２０にパーティクルが留まりやすくなり、パーティクルの流出口１６からの流出を抑制することができる。 At the boundary between the first hole portion 18 and the second hole portion 19, a step portion 20 that connects the inner wall of the first hole portion 18 and the inner wall of the second hole portion 10 is formed. As a result, even if particles are generated on the inner wall of the second hole portion 19, the particles easily stay on the stepped portion 20, and the outflow of particles from the outlet 16 can be suppressed.
　第１孔部１８の内壁は、セラミック焼結体の焼き肌面からなる。焼き肌面は、後述するように、焼成によってセラミック焼結体を得た後に加工されていない、焼成したままの表面である。この第１孔部１８の内壁は、流出口１６の近傍に位置する第１領域２１と、第１領域２１よりも本体１２の内部に位置する第２領域２２とを有する。本実施形態の第２領域２２は、第１孔部１８における第１領域２１以外の領域である。なお、第１孔部１８の内壁が焼き肌面であることは、第１孔部１８の内壁を走査型電子顕微鏡または金属顕微鏡で観察することによって確認することができる。 The inner wall of the first hole portion 18 is made of a sintered surface of a ceramic sintered body. As will be described later, the burnt surface is a surface that has not been processed after the ceramic sintered body is obtained by firing and is still fired. The inner wall of the first hole 18 has a first region 21 located near the outlet 16 and a second region 22 located inside the main body 12 rather than the first region 21. The second region 22 of the present embodiment is a region other than the first region 21 in the first hole 18. In addition, it can confirm that the inner wall of the 1st hole 18 is a burnt skin surface by observing the inner wall of the 1st hole 18 with a scanning electron microscope or a metal microscope.
　第２孔部１９の内壁は、セラミック焼結体の研削面または研磨面などの加工面からなる。研削面は、焼成によってセラミック焼結体を得た後に研削加工を行なった面である。また、研磨面は、焼成によってセラミック焼結体を得た後に研削加工を行ない、さらに研磨加工を行なった表面である。この第２孔部１９の内壁は、流入口１７の近傍に位置する第３領域２３と、第３領域２３よりも本体１２の内部に位置する第４領域２４とを有する。本実施形態の第４領域２４は、第２孔部１９における第３領域２３以外の領域である。なお、第２孔部１９の内壁が加工面であることは、第２孔部１９の内壁を走査型電子顕微鏡または金属顕微鏡で観察することによって確認することができる。 The inner wall of the second hole portion 19 is made of a processed surface such as a ground surface or a polished surface of a ceramic sintered body. The ground surface is a surface on which grinding is performed after obtaining a ceramic sintered body by firing. Further, the polished surface is a surface that is subjected to grinding after the ceramic sintered body is obtained by firing, and further subjected to polishing. The inner wall of the second hole 19 has a third region 23 located near the inflow port 17 and a fourth region 24 located inside the main body 12 more than the third region 23. The fourth region 24 of the present embodiment is a region other than the third region 23 in the second hole 19. In addition, it can confirm that the inner wall of the 2nd hole part 19 is a processed surface by observing the inner wall of the 2nd hole part 19 with a scanning electron microscope or a metal microscope.
　ところで、成膜装置１を用いる際に、貫通孔１１の内壁を構成するセラミック焼結体の表面が反応室３内でプラズマ化したガスに晒されることがある。 By the way, when the film forming apparatus 1 is used, the surface of the ceramic sintered body constituting the inner wall of the through hole 11 may be exposed to a plasma gas in the reaction chamber 3.
　一方、本実施形態においては、貫通孔１１の内壁において、第１領域２１および第２領域２２が焼き肌面からなる。この焼き肌面は、加工による損傷を受けておらず、加工面と比較して平滑な表面となっているため、焼き肌面がプラズマ化したガスに晒された際にパーティクルが脱落しにくい。したがって、第１領域２１および第２領域２２におけるパーティクルの発生を低減できる。 On the other hand, in the present embodiment, on the inner wall of the through hole 11, the first region 21 and the second region 22 are made of a burnt surface. Since this burnt skin surface is not damaged by processing and is a smooth surface as compared with the processed surface, the particles are less likely to fall off when the burnt skin surface is exposed to plasma gas. Therefore, the generation of particles in the first region 21 and the second region 22 can be reduced.
　さらに、第１領域２１における平均結晶粒径は、第２領域２２における平均結晶粒径よりも大きい。セラミック焼結体の焼き肌面における平均結晶粒径が大きいと、プラズマに腐食されやすい結晶粒界の焼き肌面における面積の割合が小さくなる。このため、焼き肌面がプラズマ化したガスに晒された際にパーティクルが脱落しにくくなる。したがって、流出口１６の近傍に位置することから第２領域２２よりもプラズマ化したガスに晒されやすい第１領域２１におけるパーティクルの発生を良好に低減できる。それ故、対象物２へのパーティクルの付着を低減し、対象物２の不良の発生を抑制することができる。 Furthermore, the average crystal grain size in the first region 21 is larger than the average crystal grain size in the second region 22. When the average crystal grain size on the surface of the ceramic sintered body is large, the ratio of the area on the surface of the sintered surface of the crystal grain boundary that is easily corroded by plasma decreases. For this reason, it becomes difficult for particles to fall off when the burnt skin surface is exposed to a plasma gas. Therefore, since it is located in the vicinity of the outlet 16, it is possible to satisfactorily reduce the generation of particles in the first region 21 that is more easily exposed to plasmad gas than the second region 22. Therefore, the adhesion of particles to the object 2 can be reduced, and the occurrence of defects in the object 2 can be suppressed.
　また、セラミック焼結体の焼き肌面における平均結晶粒径が小さいと、焼き肌面における結晶粒子の充填率が高くなるため、焼き肌面の機械的強度が高くなる。したがって、本体１２の内部に位置することから第１領域２１よりもプラズマ化したガスに晒されにくい第２領域２２において、プラズマ化したガスによる影響を低減しつつ機械的強度を高めることによって、機械的応力または熱応力に起因した本体１２の損傷を抑制することができる。 In addition, if the average crystal grain size on the surface of the ceramic sintered body is small, the filling rate of the crystal particles on the surface of the ceramic surface increases, so that the mechanical strength of the surface of the ceramic surface increases. Therefore, in the second region 22 which is located inside the main body 12 and is less exposed to the plasmad gas than the first region 21, the mechanical strength is increased while reducing the influence of the plasmad gas. Damage to the main body 12 due to mechanical stress or thermal stress can be suppressed.
　第１領域２１は、流出口１６からの距離が５ｍｍ以下の領域であることが望ましい。さらに、第１領域２１は、流出口１６からの距離が１ｍｍ以下の領域であることが望ましい。その結果、プラズマ化したガスに晒されやすい領域を第１領域２１としつつ、プラズマ化したガスに晒されにくい領域を第２領域２２とすることができるため、パーティクルの発生を良好に低減しつつ、機械的応力または熱応力に起因した本体１２の損傷を抑制することができる。 The first area 21 is desirably an area having a distance of 5 mm or less from the outlet 16. Furthermore, the first region 21 is desirably a region having a distance of 1 mm or less from the outlet 16. As a result, the region that is easily exposed to the plasma gas can be the first region 21 and the region that is not easily exposed to the plasma gas can be the second region 22. Therefore, the generation of particles can be reduced well. In addition, damage to the main body 12 due to mechanical stress or thermal stress can be suppressed.
　第１領域２１における平均結晶粒径は、第２領域２２における平均結晶粒径の１．５倍以上であることが望ましい。その結果、第１領域２１におけるパーティクルの発生を良好に低減することができる。さらに、第１領域２１における平均結晶粒径は、第２領域２２における平均結晶粒径の１０倍以下であることが望ましい。第１領域２１における平均結晶粒径は、例えば３μｍ以上２０μｍ以下である。また、第２領域２２における平均結晶粒径は、例えば２μｍ以上１０μｍ以下である。この第１領域２１および第２領域２２における平均結晶粒径は、第１領域２１および第２領域２２の表面を金属顕微鏡を用いて撮影し、この撮影画像を、画像解析装置（ニレコ社製：ＬＵＺＥＸ－ＦＳ）を用いて解析することによって求めることができる。 The average crystal grain size in the first region 21 is desirably 1.5 times or more than the average crystal grain size in the second region 22. As a result, the generation of particles in the first region 21 can be favorably reduced. Further, the average crystal grain size in the first region 21 is desirably 10 times or less than the average crystal grain size in the second region 22. The average crystal grain size in the first region 21 is, for example, 3 μm or more and 20 μm or less. The average crystal grain size in the second region 22 is, for example, 2 μm or more and 10 μm or less. The average crystal grain size in the first region 21 and the second region 22 is obtained by photographing the surfaces of the first region 21 and the second region 22 using a metal microscope, and using the photographed image as an image analysis apparatus (manufactured by Nireco Corporation: It can be determined by analyzing using (LUZEX-FS).
　また、本実施形態の貫通孔１１においては、前述した如く、第１孔部１８の内壁は焼き肌面からなり、第２孔部１９の内壁は研削面または研磨面などの加工面からなる。したがって、第２孔部１９よりも流出口１６側に位置するためプラズマ化したガスに晒されやすい第１孔部１８の内壁が焼き肌面からなることから、パーティクルの発生を良好に低減することができる。一方、第２孔部１９は、内壁が加工面からなることから、内壁が焼き肌面からなる場合と比較して、加工によって位置や形状の精度を高めることができる。したがって、第１孔部１８よりも流入口１７側に位置するためプラズマ化したガスに晒されにくい第２孔部１９において、プラズマ化したガスによる影響を低減しつつ、位置や形状の精度を高め、ガスノズル５とガス供給管４との接続不良に起因したガス漏れを抑制することができる。 Further, in the through hole 11 of the present embodiment, as described above, the inner wall of the first hole portion 18 is a burnt surface, and the inner wall of the second hole portion 19 is a processed surface such as a ground surface or a polished surface. Therefore, since the inner wall of the first hole 18 that is easily exposed to plasma gas because it is located on the outlet 16 side of the second hole 19 is made of a burnt surface, the generation of particles can be reduced well. Can do. On the other hand, since the inner wall is made of a machined surface, the second hole portion 19 can improve the accuracy of the position and shape by machining as compared with the case where the inner wall is made of a burnt surface. Therefore, in the second hole portion 19 which is located on the inlet 17 side of the first hole portion 18 and is not easily exposed to plasma gas, the influence of the plasma gas is reduced, and the position and shape accuracy are increased. Further, gas leakage due to poor connection between the gas nozzle 5 and the gas supply pipe 4 can be suppressed.
　特に、第２孔部１９においては、流入口１７の近傍に位置する第３領域２３が研削面または研磨面などの加工面からなるため、ガスノズル５とガス供給管４との接続不良に起因したガス漏れを良好に抑制することができる。第３領域２０は、流入口１７からの距離が５ｍｍ以下の領域であることが望ましい。 In particular, in the second hole portion 19, the third region 23 located in the vicinity of the inflow port 17 is formed by a processing surface such as a grinding surface or a polishing surface, and thus is caused by poor connection between the gas nozzle 5 and the gas supply pipe 4. Gas leakage can be suppressed satisfactorily. The third region 20 is preferably a region having a distance of 5 mm or less from the inflow port 17.
　また、第１領域２１における平均結晶粒径は、第３領域２３における平均結晶粒径よりも大きい。その結果、第１領域２１における平均結晶粒径を大きくすることによって前述した如くパーティクルの発生を良好に低減しつつ、第３領域２３における平均結晶粒径を小さくすることによって、機械的応力または熱応力に起因した本体１２の損傷を抑制することができる。 Further, the average crystal grain size in the first region 21 is larger than the average crystal grain size in the third region 23. As a result, by increasing the average crystal grain size in the first region 21 as described above, the generation of particles is satisfactorily reduced, while reducing the average crystal grain size in the third region 23, thereby increasing mechanical stress or heat. Damage to the main body 12 due to stress can be suppressed.
　また、本体１２の一端面１３は、セラミック焼結体の焼き肌面からなることが望ましい。その結果、プラズマ化したガスに晒されやすい一端面１３が焼き肌面からなることから、パーティクルの発生を良好に低減することができる。また、本体１２の一端面１３から貫通孔１１の第１領域２１に渡って焼き肌面が連続的に形成されていることが望ましい。その結果、パーティクルの発生を良好に低減することができる。なお、一端面１３の形状の精度を高める場合には、一端面１３を研削面または研磨面などの加工面としてもよい。この場合、パーティクルの脱落を抑制する観点から、一端面１３を研磨面とすることが望ましい。 Further, it is desirable that the one end surface 13 of the main body 12 is made of a sintered surface of a ceramic sintered body. As a result, since the one end face 13 that is easily exposed to plasma gas is a burnt surface, the generation of particles can be reduced satisfactorily. Further, it is desirable that the burnt surface is continuously formed from the one end surface 13 of the main body 12 to the first region 21 of the through hole 11. As a result, the generation of particles can be reduced favorably. In order to increase the accuracy of the shape of the one end surface 13, the one end surface 13 may be a processed surface such as a ground surface or a polished surface. In this case, it is desirable that the one end surface 13 is a polished surface from the viewpoint of suppressing the falling off of the particles.
　また、本体１２の他端面１４は、セラミック焼結体の研削面または研磨面からなることが望ましい。その結果、ガスノズル５とガス供給管４との接続不良に起因したガス漏れを良好に抑制することができる。 Further, the other end surface 14 of the main body 12 is preferably made of a ground surface or a polished surface of a ceramic sintered body. As a result, gas leakage due to poor connection between the gas nozzle 5 and the gas supply pipe 4 can be satisfactorily suppressed.
　＜ガスノズルの製造方法＞
  次に、前述したガスノズル５の製造方法を、図３および図４を参照しつつ説明する。 <Manufacturing method of gas nozzle>
Next, the manufacturing method of the gas nozzle 5 mentioned above is demonstrated, referring FIG. 3 and FIG.
　（１）まず、図３および図４に示すように、前述した本体１２の貫通孔１１が形成される前のセラミック焼結体である本体用焼結体２５を作製する。具体的には、例えば以下のように行なう。 (1) First, as shown in FIGS. 3 and 4, a main body sintered body 25 which is a ceramic sintered body before the through hole 11 of the main body 12 is formed is prepared. Specifically, for example, the following is performed.
　まず、セラミック粉末に純水と有機バインダーを加えた後、ボールミルで湿式混合してスラリーを作製する。次に、スラリーをスプレードライにて造粒し、セラミック粉末を形成する。次に、セラミック粉末を用いて、金型プレス法または冷間静水圧プレス成形法（ＣＩＰ成形法）などの成形法を用いて所定の形状に成形して図３（ａ）に示した円柱状の成形体２６を得る。次に、図３（ｂ）に示すように、切削加工を用いて、前述した第１孔部１８となる、一端面１３に開口した凹部２７を成形体２６に形成する。次に、図４（ａ）に示すように、大気雰囲気中または酸素雰囲気中のいずれかにて例えば１４００℃以上２０００℃以下で焼成する。以上のようにして、図４（ｂ）に示した本体用焼結体２５を得ることができる。この本体用焼結体２５において、一端面１３、他端面１４、側面１５および凹部２７の内壁といった表面は、焼成後に加工されておらず、焼き肌面となっている。 First, pure water and an organic binder are added to the ceramic powder, and then wet mixed with a ball mill to prepare a slurry. Next, the slurry is granulated by spray drying to form a ceramic powder. Next, the ceramic powder is molded into a predetermined shape using a molding method such as a die pressing method or a cold isostatic pressing method (CIP molding method), and the cylindrical shape shown in FIG. The molded body 26 is obtained. Next, as shown in FIG. 3 (b), a recess 27 that opens to the one end surface 13 that forms the first hole 18 described above is formed in the molded body 26 by cutting. Next, as shown in FIG. 4A, firing is performed at, for example, 1400 ° C. or more and 2000 ° C. or less in either an air atmosphere or an oxygen atmosphere. As described above, the main body sintered body 25 shown in FIG. 4B can be obtained. In the main body sintered body 25, the surfaces such as the one end surface 13, the other end surface 14, the side surface 15, and the inner wall of the concave portion 27 are not processed after firing, and have a burnt surface.
　本実施形態において、成形体２６の焼成は、図４（ａ）に示すように、凹部２７が開口した一端面１３を上側として露出させつつ、焼成炉の載置台２８上に成形体２６を載置した状態で行なう。その結果、成形体２６の焼成の際に、成形体２６の上方から熱が加わるため、凹部２７の内壁においては、一端面１３の近傍に位置する第１領域２１に、第１領域２１よりも成形体２６の内部に位置する第２領域２２と比較して、大きな熱が加わりやすい。 In the present embodiment, as shown in FIG. 4 (a), the molded body 26 is fired by placing the molded body 26 on the mounting table 28 of the firing furnace while exposing the one end surface 13 with the recess 27 opened as an upper side. It is done in the state. As a result, since heat is applied from above the molded body 26 during the firing of the molded body 26, the inner wall of the recess 27 has a first region 21 located near the one end surface 13 in the first region 21 than the first region 21. Compared with the second region 22 located inside the molded body 26, large heat is likely to be applied.
　ここで、本体用焼結体２５としてイットリア焼結体、イットリウム・アルミニウム・ガーネット焼結体、スピネル焼結体または高純度アルミナ焼結体を形成する場合には、成形体２６を焼成する際に液相焼結が生じる。このため、第２領域２２よりも大きな熱が加わる第１領域２１の結晶は、第２領域２２よりも大きく成長しやすい。その結果、本体用焼結体２５の凹部２７の内壁において、第１領域２１における平均結晶粒径を第２領域２２における平均結晶粒径よりも大きくすることができる。 Here, when the yttria sintered body, the yttrium / aluminum / garnet sintered body, the spinel sintered body, or the high-purity alumina sintered body is formed as the main body sintered body 25, the molded body 26 is fired. Liquid phase sintering occurs. For this reason, the crystal of the first region 21 to which heat larger than that of the second region 22 is applied is likely to grow larger than that of the second region 22. As a result, the average crystal grain size in the first region 21 can be made larger than the average crystal grain size in the second region 22 on the inner wall of the recess 27 of the main body sintered body 25.
　特に、直径が０．１ｍｍ以上２ｍｍ以下と小さい第１孔部１８を形成する場合には、第１孔部１８となる凹部２７の直径も小さくする必要があるため、凹部２７内にて空気が流動しにくくなる。したがって、成形体２６の焼成の際に、凹部２７の内壁における熱の加わり方が不均一となりやすく、第１領域２１に加わる熱が第２領域２２に加わる熱よりも大きくなりやすい。このため、本体用焼結体２５の凹部２７の内壁において、第１領域２１における平均結晶粒径を第２領域２２における平均結晶粒径よりも大きくしやすい。 In particular, when the first hole 18 having a diameter as small as 0.1 mm or more and 2 mm or less is formed, it is necessary to reduce the diameter of the recess 27 serving as the first hole 18. It becomes difficult to flow. Therefore, when the molded body 26 is baked, the heat applied to the inner wall of the recess 27 is likely to be uneven, and the heat applied to the first region 21 is likely to be greater than the heat applied to the second region 22. Therefore, the average crystal grain size in the first region 21 is likely to be larger than the average crystal grain size in the second region 22 on the inner wall of the recess 27 of the main body sintered body 25.
　また、凹部２７は、一端面１３と反対側の端部に底面を有しており、本体１２を貫通していない。その結果、凹部２７内を空気が流動しにくくなる。したがって、本体用焼結体２５の凹部２７の内壁において、第１領域２１における平均結晶粒径を第２領域２２における平均結晶粒径よりも大きくしやすい。 The recess 27 has a bottom surface at the end opposite to the one end surface 13 and does not penetrate the main body 12. As a result, it becomes difficult for air to flow in the recess 27. Therefore, the average crystal grain size in the first region 21 is likely to be larger than the average crystal grain size in the second region 22 on the inner wall of the recess 27 of the main body sintered body 25.
　また、成形体２６を形成する際の成形方法としては、ＣＩＰ成形法を用いることが望ましい。ＣＩＰ成形法によれば、成形時の圧力が均一に加わるため、成形体２６の密度を均一にすることができる。したがって、成形体２６を焼成する際に、加わる温度に応じて結晶粒子が均一に成長するため、前述した如く、第１領域２１に第２領域２２よりも大きな熱を加えることによって、第１領域２１における平均結晶粒径を第２領域２２における平均結晶粒径よりも大きくしやすい。 In addition, as a molding method for forming the molded body 26, it is desirable to use a CIP molding method. According to the CIP molding method, since the pressure during molding is uniformly applied, the density of the molded body 26 can be made uniform. Therefore, when the molded body 26 is fired, crystal grains grow uniformly according to the applied temperature. As described above, the first region 21 is heated by applying heat larger than that of the second region 22 to the first region 21. The average crystal grain size in 21 is easily made larger than the average crystal grain size in the second region 22.
　（２）本体用焼結体２５に貫通孔１１を形成することによって、本体用焼結体２５を本体１２として、図２に示したガスノズル５を作製する。具体的には例えば以下のように行なう。 (2) By forming the through-hole 11 in the main body sintered body 25, the main body sintered body 25 is used as the main body 12, and the gas nozzle 5 shown in FIG. Specifically, for example, the following is performed.
　研削加工を用いて、本体用焼結体２５の他端面１４側から孔加工を行ない、他端面１４に開口するとともに凹部２７とつながった第２孔部１９を本体用焼結体２５に形成する。これによって、凹部２７が第１孔部１８となり、第１孔部１８および第２孔部１９によって構成される貫通孔１１を形成することができる。また、研削加工を用いて、他端面１４を研削して研削面とする。その結果、本体用焼結体２５を本体１２とすることができる。なお、研削加工として超音波加工を用いてもよい。 Hole processing is performed from the other end surface 14 side of the main body sintered body 25 using grinding, and the second hole portion 19 that opens to the other end surface 14 and is connected to the recess 27 is formed in the main body sintered body 25. . Accordingly, the recess 27 becomes the first hole 18, and the through-hole 11 constituted by the first hole 18 and the second hole 19 can be formed. Moreover, the other end surface 14 is ground by using a grinding process to obtain a ground surface. As a result, the main body sintered body 25 can be the main body 12. In addition, you may use ultrasonic processing as a grinding process.
　本工程においては、本体用焼結体２５の凹部２７からなる第１孔部１８の内壁に研削加工や研磨加工などの加工を行なわない。その結果、第１孔部１８の内壁を焼き肌面としつつ、第１孔部１８の内壁においても、本体用焼結体２５の第１領域２１および第２領域２２における平均結晶粒径を維持することができる。したがって、第１領域２１における平均結晶粒径を第２領域２２における平均結晶粒径よりも大きくすることができる。 In this step, the inner wall of the first hole portion 18 formed of the concave portion 27 of the main body sintered body 25 is not subjected to processing such as grinding or polishing. As a result, the average crystal grain size in the first region 21 and the second region 22 of the main body sintered body 25 is maintained on the inner wall of the first hole 18 while the inner wall of the first hole 18 is a burnt surface. can do. Therefore, the average crystal grain size in the first region 21 can be made larger than the average crystal grain size in the second region 22.
　また、本工程において、一端面１３に研削加工または研磨加工などの加工を行なわないことによって、一端面１３を焼き肌面とすることができる。この場合、焼き肌面は、本体１２の一端面１３から貫通孔１１の第１領域２１に渡って連続的に形成される。なお、一端面１３の形状の精度を高める場合には、一端面１３に研削加工または研磨加工などの加工を行なってもよい。この場合、本体用焼結体２５の長手方向に沿った加工量は、例えば０．５ｍｍ以上２ｍｍ以下であることが望ましい。その結果、第１領域２１を本体１２に残存させることができる。 Further, in this step, the one end surface 13 can be made to be a burnt skin surface by not performing processing such as grinding or polishing on the one end surface 13. In this case, the grilled surface is continuously formed from the one end surface 13 of the main body 12 to the first region 21 of the through hole 11. In addition, when improving the accuracy of the shape of the one end surface 13, the end surface 13 may be subjected to processing such as grinding or polishing. In this case, the processing amount along the longitudinal direction of the main body sintered body 25 is desirably, for example, not less than 0.5 mm and not more than 2 mm. As a result, the first region 21 can remain in the main body 12.
　また、第２孔部１９は研削加工によって形成されるため、第２孔部１９の内壁は研削面となる。なお、研削加工を用いて第２孔部１９を形成した後に、第２孔部１９の内壁に研磨加工を行なうことによって、第２孔部１９の内壁を研磨面とすることができる。また、研削加工を用いて他端面１４を研削面とした後に、他端面１４に研磨加工を行なうことによって、他端面１４を研磨面とすることができる。 In addition, since the second hole 19 is formed by grinding, the inner wall of the second hole 19 becomes a ground surface. In addition, after forming the 2nd hole part 19 using a grinding process, the inner wall of the 2nd hole part 19 can be made into a grinding | polishing surface by grind | polishing the inner wall of the 2nd hole part 19. FIG. Moreover, after making the other end surface 14 into a grinding surface using grinding, the other end surface 14 can be used as a polishing surface by polishing the other end surface 14.
　以上のようにして、図２に示したガスノズル５を作製することができる。 As described above, the gas nozzle 5 shown in FIG. 2 can be manufactured.
　本発明は前述した実施形態に限定されるものではなく、本発明の要旨を逸脱しない範囲において種々の変更、改良、組合せ等が可能である。 The present invention is not limited to the above-described embodiments, and various changes, improvements, combinations, and the like can be made without departing from the gist of the present invention.
　例えば、前述した実施形態において、ガスノズルを成膜装置に用いた構成を例に説明したが、ガスノズルは他の半導体製造装置や液晶製造装置に用いてもよく、例えばエッチング装置に用いてもよい。 For example, in the above-described embodiment, the configuration in which the gas nozzle is used in the film forming apparatus has been described as an example. However, the gas nozzle may be used in another semiconductor manufacturing apparatus or liquid crystal manufacturing apparatus, for example, an etching apparatus.
１　　成膜装置
２　　対象物
３　　反応室
４　　ガス供給管
５　　ガスノズル
６　　内部電極
７　　保持部材
８　　バイアス電源
９　　コイル
１０　電源
１１　貫通孔
１２　本体
１３　一端面
１４　他端面
１５　側面
１６　流出口
１７　流入口
１８　第１孔部
１９　第２孔部
２０　段差部
２１　第１領域
２２　第２領域
２３　第３領域
２４　第４領域
２５　本体用焼結体
２６　成形体
２７　凹部
２８　載置台 DESCRIPTION OF SYMBOLS 1 Film-forming apparatus 2 Object 3 Reaction chamber 4 Gas supply pipe 5 Gas nozzle 6 Internal electrode 7 Holding member 8 Bias power supply 9 Coil 10 Power supply 11 Through-hole 12 Main body 13 One end surface 14 The other end surface 15 Side surface 16 Outlet 17 Inlet 18 First 1 hole part 19 2nd hole part 20 step part 21 1st field 22 2nd field 23 3rd field 24 4th field 25 sintered body 26 for main body molded object 27 recessed part 28 mounting table

Claims (8)

  1. 　ガスが流れる貫通孔が形成されたセラミック焼結体からなる柱状の本体を備え、
    該本体の一端面には、前記貫通孔における前記ガスの流出口が形成されており、
    前記貫通孔の内壁は、前記流出口の近傍に位置する第１領域と該第１領域よりも前記本体の内部に位置する第２領域とを有し、
    前記第１領域および前記第２領域は、前記セラミック焼結体の焼き肌面からなり、
    前記第１領域における平均結晶粒径は、前記第２領域における平均結晶粒径よりも大きいガスノズル。     A columnar body made of a ceramic sintered body in which a through-hole through which gas flows is formed,
    An outlet of the gas in the through hole is formed on one end surface of the main body,
    The inner wall of the through hole has a first region located in the vicinity of the outlet and a second region located inside the main body rather than the first region,
    The first region and the second region are composed of a sintered surface of the ceramic sintered body,
    The gas nozzle in which the average crystal grain size in the first region is larger than the average crystal grain size in the second region.
  2. 　請求項１に記載のガスノズルにおいて、
    前記セラミック焼結体は、イットリア焼結体、イットリウム・アルミニウム・ガーネット焼結体、スピネル焼結体またはアルミナ純度が９９．５質量％以上であるアルミナ焼結体からなるガスノズル。     The gas nozzle according to claim 1, wherein
    The ceramic sintered body is a gas nozzle comprising an yttria sintered body, an yttrium / aluminum / garnet sintered body, a spinel sintered body, or an alumina sintered body having an alumina purity of 99.5% by mass or more.
  3. 　請求項１に記載のガスノズルにおいて、
    前記第１領域は、前記流出口からの距離が５μｍ以下の領域であるガスノズル。     The gas nozzle according to claim 1, wherein
    The gas nozzle in which the first region is a region having a distance of 5 μm or less from the outflow port.
  4. 　請求項１に記載のガスノズルにおいて、
    前記第１領域における平均結晶粒径は、前記第２領域における平均結晶粒径の１．５倍以上１０倍以下であるガスノズル。     The gas nozzle according to claim 1, wherein
    The gas nozzle in which the average crystal grain size in the first region is 1.5 to 10 times the average crystal grain size in the second region.
  5. 　請求項１に記載のガスノズルにおいて、
    前記本体の前記一端面は、前記セラミック焼結体の焼き肌面からなるガスノズル。     The gas nozzle according to claim 1, wherein
    The gas nozzle in which the one end surface of the main body is a burnt surface of the ceramic sintered body.
  6. 　請求項１に記載のガスノズルにおいて、
    前記本体の他端面には、前記貫通孔における前記ガスの流入口が形成されており、
    前記貫通孔の内壁は、前記流入口の近傍に位置する第３領域を有し、
    該第３領域は、前記セラミック焼結体の研削面または研磨面からなり、
    前記第１領域における平均結晶粒径は、前記第３領域における平均結晶粒径よりも大きいガスノズル。     The gas nozzle according to claim 1, wherein
    On the other end surface of the main body, an inlet for the gas in the through hole is formed,
    The inner wall of the through hole has a third region located in the vicinity of the inflow port,
    The third region comprises a ground surface or a polished surface of the ceramic sintered body,
    The gas nozzle in which the average crystal grain size in the first region is larger than the average crystal grain size in the third region.
  7. 　請求項６に記載のガスノズルにおいて、
    前記本体の他端面は、前記セラミック焼結体の研削面または研磨面からなるガスノズル。     The gas nozzle according to claim 6.
    The other end surface of the main body is a gas nozzle comprising a ground surface or a polished surface of the ceramic sintered body.
  8. 　反応室と、該反応室内に前記ガスが流出する請求項１に記載のガスノズルと、前記ガスを放電によってプラズマ化させる放電部材とを備えたプラズマ装置。 A plasma apparatus comprising: a reaction chamber; the gas nozzle according to claim 1 through which the gas flows into the reaction chamber; and a discharge member that converts the gas into plasma by discharge.
PCT/JP2013/084380 2013-01-30 2013-12-21 Gas nozzle and plasma device employing same WO2014119177A1 (en)

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